Investigation of Pb-Mg-Nb-O pyrochlore thin films for tunable material

PMN thin films have been investigated as a feasible material for tunable microwave applications. PMN thin films were deposited by RF magnetron sputtering from Pb₆MgNb₆O₂₂ ceramic target on platinized Si substrates. The crystallinity, thickness, surface morphology, dielectric property, and voltage tunable properties of thin films were investigated by means of X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), and an impedance analyzer. The influences of sputtering substrate temperature and post-annealing on the tunable dielectric properties of thin films were investigated. Increasing the sputtering substrate temperature and annealing temperature can significantly increase tunability; however, these relations had the limitation that overly annealing temperature degraded the tunability of the thin film. A tunability of 38% at 1100 kV/cm of dc bias field under 1 MHz was achieved for a sample sputtered at 550 °C and annealed at 700 °C.     

Influence of deposition parameters and heat treatment on the NO2 sensing properties of nanostructured indium tin oxide thin film

Highly oriented and transparent indium tin oxide (ITO) films have been deposited onto glass substrates by radio frequency magnetron sputtering at 648 K, under an oxygen partial pressure of 1 Pa. The effect of the sputtering power and annealing was studied. Transmission was measured with a double beam spectrometer and electrical analysis using four probe and Hall effect setup. Structural characterization of the films was done by X-ray diffraction. Characterization of the coatings revealed an electrical resistivity below 6.5 × 10^− 3 Ω cm. The ITO films deposited at 648 K were amorphous, while the crystallinity improved after annealing at 700 K. The optical transmittance of the film was more than 80% in the visible region. The surface morphology examined by scanning electron microscopy appears to be uniform over the entire surface area, after annealing. The NO₂ sensing properties of the ITO films were investigated. At a working temperature of 600 K, the ITO sensor showed high sensitivity to NO₂ gas, at concentrations lower than 50 ppm.     

Annealing dependence of residual stress and optical properties of TiO2 thin film deposited by different deposition methods

Titanium oxide (TiO(2)) thin films were prepared by different deposition methods. The methods were E-gun evaporation with ion-assisted deposition (IAD), radio-frequency (RF) ion-beam sputtering, and direct current (DC) magnetron sputtering. Residual stress was released after annealing the films deposited by RF ion-beam or DC magnetron sputtering but not evaporation, and the extinction coefficient varied significantly. The surface roughness of the evaporated films exceeded that of both sputtered films. At the annealing temperature of 300 degrees C, anatase crystallization occurred in evaporated film but not in the RF ion-beam or DC magnetron-sputtered films. TiO(2) films deposited by sputtering were generally more stable during annealing than those deposited by evaporation.     

Effects of heat treatment on properties of ITO films prepared by rf magnetron sputtering

Indium tin oxide (ITO) films were deposited on glass substrates by rf magnetron sputtering using a ceramic target (In₂O₃-SnO₂, 90-10 wt%) without extra heating. The post annealing was done in air and in vacuum, respectively. The effects of annealing on the structure, surface morphology, optical and electrical properties of the ITO films were studied. The results show that the increase of the annealing temperature improves the crystallinity of the films, increases the surface roughness, and improves the optical and electrical properties. The transmittance of the films in visible region is increased over 90% after the annealing process in air or in vacuum. The resistivity of the films deposited is about 8.125×10⁻⁴ Ω cm and falls down to 2.34×10⁻⁴ Ω cm as the annealing temperature is increased to 500°C in vacuum. Compared with the results of the ITO films annealed in air, the properties of the films annealed in vacuum is better.     

Influence of rapid thermal annealing on surface texture-etched Al-doped ZnO films prepared by various magnetron sputtering methods

The influence of rapid thermal annealing (RTA) on surface texture formation as well as the light management obtainable by wet-chemically etching was investigated for transparent conducting Al-doped ZnO (AZO) thin films prepared by various types of magnetron sputtering deposition (MSD) with an oxide target. Texture-etched AZO films prepared by an r.f. (13.56 MHz) power-superimposed d.c. magnetron sputtering deposition (rf + dc-MSD) exhibited a higher haze value than found in equivalent films prepared by d.c. MSD. The order that the RTA treatment and the etching were conducted considerably affected the obtainable surface texture. Conducting the etching after a heat treatment with RTA in air resulted in larger etch pits as well as higher haze values than were obtained in AZO films that were etched before the RTA. A high haze value generally above 70% in the range from visible to near infrared (at wavelengths up to 1200 nm) was obtained in texture-etched AZO thin films that were prepared by rf + dc-MSD and etched after RTA at a temperature of 500 °C for 3 min.     

Microstructure and properties of Al-doped ZnO thin films by nonreactive DC magnetron sputtering at room temperature following rapid thermal annealing

A series of Al-doped ZnO (AZO) thin films deposited by nonreactive DC magnetron sputtering at room temperature following rapid thermal annealing was studied to examine the influence of these Al doping concentration, sputtering power and annealing temperature on their microstructure, electrical and optical transport properties. AZO thin films with Al dopant of 3 wt% were oriented more preferentially along the (002) direction, bigger grain size and lower electrical resistivity The resistivity of AZO films decreases with the increase of Al content from 1 to 3 wt%, sputtering power from 60 to 100 W and the annealing temperature from 50 to 250 °C. Sputtering power and annealing had some effect on the average transmittance of AZO thin films. For AZO thin films with Al doping level of 3 wt%, the lowest electrical resistivity of 5.3 × 10⁻⁴ Ω cm and the highest optical transmittance of 88.7% could gain when the sputtering power was 100 W and the annealing temperature was 200 °C or above.     

Effect of processing conditions on microstructure and electrical characteristics of Ni thin films

Ni thin films with an intermediate layer of Cr were prepared by using dc magnetron sputtering under different conditions. Effects of deposition temperature, post-deposition annealing on the microstructure and the electrical characteristics were investigated. The relationship between film microstructure and its resistivity was analyzed. It was found that the crystal grains aggregated into large ones when the deposition temperature reached or exceeded 150 °C. This could be explained that high deposition temperature conduced high activation energy, which increased surface mobility of the adatoms. Annealing treatments resulted in the densification of the films. Resistivity of the films strongly depended on grain size and crystallinity. The influence of Cr intermediate layer on the resistivity was also discussed. Compared to annealing treatment, the deposition temperature exhibited larger controlling effect on film resistivity.     

磁控溅射硅钼薄膜的抗氧化性能研究

用射频磁控溅射法在单晶Si基体上制备了硅钼薄膜,对薄膜进行真空退火处理以及高温氧化实验,借助SEM和X射线衍射仪(XRD)等仪器对退火前后的薄膜以及高温氧化后的薄膜进行了分析。结果表明沉积态的硅钼薄膜为非晶态,高温真空退火使薄膜由非晶态转变为晶态,致密的复合氧化物是硅钼薄膜具有良好的抗氧化性能的主要原因。     

Annealing effect on crystallization behavior of cubic MgxZn1−xO films on A-plane and M-plane sapphire

Cubic Mg_xZn_1−xO thin films with Mg composition around 70% were deposited on A-plane and M-plane sapphire substrates by rf-reactive magnetron sputtering. Measured structural and optical properties of these thin films indicated an optimal annealing temperature of 700 °C which produced high quality cubic MgZnO thin films on both substrates. Moreover, when the annealing temperature exceeded 750 °C, a much rougher surface resulted, and several large mosaic particles on the surface of the annealed films appeared. From EDX results, the Mg composition was lower than that found in other sections of the annealed films. We attributed this to thermally induced reconstruction of the crystallites. This phenomenon was more obvious for annealed MgZnO films on A-plane sapphire than that on M-plane sapphire. Thermal expansion mismatch with the substrate is the principal reason.     

Electrical,morphological and structural properties of RF magnetron sputtered Mo thin films for application in thin film photovoltaic solar cells

Molybdenum (Mo) thin films were deposited using radio frequency magnetron sputtering, for application as a metal back contact material in “substrate configuration” thin film solar cells. The variations of the electrical, morphological, and structural properties of the deposited films with sputtering pressure, sputtering power and post-deposition annealing were determined. The electrical conductivity of the Mo films was found to increase with decreasing sputtering pressure and increasing sputtering power. X-ray diffraction data showed that all the films had a (110) preferred orientation that became less pronounced at higher sputtering power while being relatively insensitive to process pressure. The lattice stress within the films changed from tensile to compressive with increasing sputtering power and the tensile stress increased with increasing sputtering pressure. The surface morphology of the films changed from pyramids to cigar-shaped grains for a sputtering power between 100 and 200 W, remaining largely unchanged at higher power. These grains were also observed to decrease in size with increasing sputtering pressure. Annealing the films was found to affect the resistivity and stress of the films. The resistivity increased due to the presence of residual oxygen and the stress changed from tensile to compressive. The annealing step was not found to affect the crystallisation and grain growth of the Mo films.     

射频磁控溅射法制备碲化铅薄膜的X射线衍射分析

采用射频磁控溅射法,在单面抛光的Si(111)衬底上制备了PbTe薄膜,利用X射线衍射法分析了溅射工艺参数如溅射功率、溅射时间、衬底温度以及退火温度对PbTe薄膜的结晶质量的影响。结果表明:在溅射功率为30W,溅射时间为10 min,衬底未加热时制备的薄膜具有最好的〈100〉方向的择优取向性;退火处理可以改善薄膜的结晶质量,并且退火温度越高,薄膜的结晶质量越好。     

Influence of annealing temperature on the structural, mechanical and wetting property of TiO2 films deposited by RF magnetron sputtering

TiO₂ films have been deposited on silicon substrates by radio frequency magnetron sputtering of a pure Ti target in Ar/O₂ plasma. The TiO₂ films deposited at room temperature were annealed for 1 h at different temperatures ranging from 400 °C to 800 °C. The structural, morphological, mechanical properties and the wetting behavior of the as deposited and annealed films were obtained using Raman spectroscopy, atomic force microscopy, transmission electron microscopy, nanoindentation and water contact angle (CA) measurements. The as deposited films were amorphous, and the Raman results showed that anatase phase crystallization was initiated at annealing temperature close to 400 °C. The film annealed at 400 °C showed higher hardness than the film annealed at 600 °C. In addition, the wettability of film surface was enhanced with an increase in annealing temperature from 400 °C to 800 °C, as revealed by a decrease in water CA from 87° to 50°. Moreover, the water CA of the films obtained before and after UV light irradiation revealed that the annealed films remained more hydrophilic than the as deposited film after irradiation.     

Nanocrystalline SnO2 and Au:SnO2 thin films prepared by direct current magnetron reactive sputtering

Nanocrystalline pure and gold doped SnO₂(Au:SnO₂) films were prepared on unheated glass substrates by dc magnetron reactive sputtering and, subsequently, the as deposited films were annealed in air. The films structure, surface morphology, photoluminescence, electrical and optical properties were investigated. After annealing the as deposited SnO₂ films, crystallinity increased and the surface roughness decreased. The intensity of PL peaks increases sharply with the annealing temperature. The optical transmittance of the films was around 89% after annealing the as deposited SnO₂ films at 450 °C. The as deposited Au:SnO₂ films show better crystallinity than the as deposited SnO₂ films, the average grain size was around 4.4 nm. The emission peaks of Au:SnO₂ films are slightly blue shifted as compare to undoped SnO₂ films. The Au:SnO₂ films show the lowest electrical resistivity of 0.001 Ωcm with optical transmittance of 76%, after annealing at 450 °C.     

Dielectric properties of DC reactive magnetron sputtered Al2O3 thin films

Alumina (Al₂O₃) thin films were sputter deposited over well-cleaned glass and Si < 100 > substrates by DC reactive magnetron sputtering under various oxygen gas pressures and sputtering powers. The composition of the films was analyzed by X-ray photoelectron spectroscopy and an optimal O/Al atomic ratio of 1.59 was obtained at a reactive gas pressure of 0.03 Pa and sputtering power of 70 W. X-ray diffraction results revealed that the films were amorphous until 550 °C. The surface morphology of the films was studied using scanning electron microscopy and the as-deposited films were found to be smooth. The topography of the as-deposited and annealed films was analyzed by atomic force microscopy and a progressive increase in the rms roughness of the films from 3.2 nm to 4.53 nm was also observed with increase in the annealing temperature. Al-Al₂O₃-Al thin film capacitors were then fabricated on glass substrates to study the effect of temperature and frequency on the dielectric property of the films. Temperature coefficient of capacitance, AC conductivity and activation energy were determined and the results are discussed.     

Preparation and properties of Mg0.2Zn0.8O:Al UV transparent conducting thin films deposited by RF magnetron sputtering at room temperature with rapid annealing

Mg_0.2Zn_0.8O:Al UV transparent conducting thin films were deposited by RF magnetron sputtering at room temperature with a rapid annealing process. Effects of sputtering power, argon gas pressure and annealing temperature on structure, optical and electrical properties of Mg_0.2Zn_0.8O:Al films were investigated. The experimental results show that Mg_0.2Zn_0.8O:Al thin films exhibit high preferred c-axis-orientation. The sputtering power, argon gas pressure and annealing temperature all exert a strong influence on the electrical resistivity of Mg_0.2Zn_0.8O:Al thin films due to the variation of carrier concentration and mobility in films derived from the change of effective doping and crystallinity. The lowest electrical resistivity of Mg_0.2Zn_0.8O:Al thin films is 3.5 × 10⁻³ Ω·cm when the sputtering power is 200 W, the argon gas pressure is 2.0 Pa and the annealing temperature is above 500 °C. The transparent spectrum range of Mg_0.2Zn_0.8O:Al thin films extend to ultraviolet band and the optical transmittance is between 80 and 90%, but the sputtering power, argon gas pressure and annealing temperature all exert little influence on optical transmittance.     

In-situ fabrication and performance optimization of CIGS thin film deposited by ion-beam sputtering without post-selenization

Cu(In, Ga)Se₂ thin films were fabricated by an in situ fabrication process of ion beam sputtering deposition without post-selenization. X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy and four-point probe technique were used to study the microstructures, surface morphology, composition and electrical properties, respectively. The results show that the films grown above 400 °C are of chalcopyrite structure and Cu (In_0.7Ga_0.3) Se₂ thin film was obtained at annealing temperature of 550 °C. With the increase in annealing temperature, the resistivity of the films decreases while the component is nearly steady. The degree of crystallization of the thin films increased at first with increasing of the annealing time and then decreased with the annealing time increasing further. It was demonstrated that the structural and electrical properties of the films improved significantly with adding selenium amount by sputtering selenium.     

Influence of deposition parameters on preferred orientation of RF magnetron sputtered BST thin films

Ba_0.65Sr_0.35TiO₃ (BST) thin films have been deposited by radio frequency magnetron sputtering. The effects of the deposition parameters on the crystallization and microstructure of BST thin films were investigated by X-ray diffraction and field emission scanning electron microscopy, respectively. The crystallization behavior of these films was apparently affected by the substrate temperature, annealing temperature and sputtering pressure. The as-deposited thin films at room temperature were amorphous. However, the improved crystallization is observed for BST thin films deposited at higher temperature. As the annealing temperature increased, the dominant X-ray diffraction peaks became sharper and more intense. The dominant diffraction peaks increased with the sputtering pressures increasing as the films deposited at 0.37–1.2 Pa. With increasing the sputtering pressure up to 3.9 Pa, BST thin films had the (110) + (200) preferred orientation. Possible correlations of the crystallization with changes in the sputtering pressure were discussed. The SEM morphologies indicated the film was small grains, smooth, and the interface between the film and the substrate was sharp and clear.     

Radio frequency sputtered zinc oxide thin films with application to metal-semiconductor-metal photodetectors

Zinc oxide (ZnO) films were successfully deposited on silicon, silicon dioxide, and glass substrates by radio frequency magnetron sputtering at different deposition conditions. Field emission scanning electron microscopy, X-ray photoelectron spectroscopy, transmission and photoluminescence measurements were employed to analyze the effect of the deposition conditions and the postdeposition annealing treatment on the surface morphology, structure, chemical deposition and optical properties of ZnO thin films. It was found that the thickness of ZnO films decreased with increased ratio of oxygen/argon and increased temperature. The crystalline and stoichiometric quality of the film was improved by depositing at high temperature and low pressure. Crystals formed more tightly and uniformly with heat treatment under air ambient. The dark current of the ZnO metal-semiconductor-metal photodetector was reduced from 3.06 μA to 96.5 nA at 5 V after postdeposition annealing when compared with that of as-deposited ZnO. Its magnitude was found to be at least two orders lower than that of the as-deposited sample.     

Effects of hydrogen annealing on the structural, optical and electrical properties of indium-doped zinc oxide films

Indium-doped zinc oxide (IZO) films were fabricated by radio-frequency magnetron sputtering. The effects of hydrogen annealing on the structural, optical and electrical properties of the IZO films were investigated. The hydrogen annealing may deteriorate the crystallinity of the films. The surfaces of the films would be damaged when the annealing temperature was higher than 350 °C. After the annealing, the surface roughness of the films would decrease, and high transparency of 80–90% in the visible and near-infrared wavelength would be kept. Meanwhile, the resistivity decreased from 1.25 × 10⁻³ Ωcm of the deposited films to 6.70 × 10⁻⁴ Ωcm of the annealed films. The work function of the IZO films may be modulated between 4.6 and 4.98 eV by varying the hydrogen annealing temperature and duration.     

Effect of annealing on the composition, structure and mechanical properties of carbon nitride films deposited by middle-frequency magnetron sputtering

Carbon nitride films were deposited by middle-frequency reactive magnetron sputtering and annealed at different temperatures in nitrogen ambient. X-ray photoelectron spectroscopy, Raman scattering, transmission electron microscopy, and nano-indenter were used to characterize the as-deposited and annealed films. The analysis showed that annealing resulted in the dissociation of N and C in the films. The dissociation of C happened after 500 °C and lagged behind that of N. With the increase of annealing temperature, the disorder of sp² C decreased and the films were gradually graphitized. The microstructure changed from amorphous to fullerene-like CN_x with the annealing temperature increasing to 500 °C, and then to nitridized graphite nanocrystals at 600 °C. The graphitization resulted in a drastic decreasing of hardness and modulus of the films.